ISO 03262-17-2024.docx
5>×SOInternationa1.StandardISo326217Secondedition2024-01ExtendersSpecificationsandmethodsoftest一PARCiMtatedca1.ciumsi1.icateMaturesdechargeSpecificationsetmethodes(TeSSQiPartie17:Si1.icatedeca1.ciumprecipiteReferencenumberISO3262-172024(en)COPYRIGHTPROTECTEDDOCUMENT©ISO2024WintG<hcdBdHUWwdotherwiseCrW4WMrtiwcmbxtt11)ni(WkJhrtRinkHimftWr1.9Htumcnpyip<?IHdiCnticnma),theinternetoranintranet,withoutpriorwrittenpermission.Permissiononber<?qucste<ifromeitherISOattheaddressbe1.oworISOsmemberbodyinthecountryoftherequester.b,Vyfrfiandonnet8CH-1214Vcmicr,GenevaPhoae:*41227490111聊独te:薪括嬴OQrgPub1.ishedinSwitzer1.andContentsforewordC5Unnp11.3.1Termsanddefinitions45RequireinentsandtestmethodsSamp1.ing26Determinationofsi1.icacontent6.1.26.2263Apparatus6.4Phce<Ture6.4.1Numberofdeterminations36.4.2Testportion,46.4.3Determinationo.(.thetoU1.1.QSSf1.nignition6.5Expressionofresu1.ts576.65DeterminationnftheCcmnCqiticnhvSnectrometrv7.1Princip1.e57.26羽Apprgt1.1.1.QPtoceaure7.4.1Preparationofstandardmatchingso1.utions7.4.2Spectrometricmeasurement77.4.3辆区的HB冷IfeStSO1.UIiOn7.57,SDetermInat1.onExpressionofresu1.ts.89苑:E8M!Wi8)ntforcachC1.enWn1.7.6Precision9811pterminntinn11frecirip11nsieve8.1Princip1.e108.2Nfateria1.s.10HApparatus.P11eure8.41Nubootdeterminations-.8StpIn.",10.105688.8cpress1.onDfeWfiWonPrecisionTestreportHiForewordISO(theInternationa1.OrganizationforStandardization)isaWOHdwidefederationofnationa1.standardsIMdIiest触UimatbnnbtidM明岷IWnribefPrbPdNMEtetfndtiOna1.Staudd<B-Mirtob1.1.ytechafrft1.ctouciihitoaghhasbeenestab1.ishedhastherighttoberepresentedonthatcommittee.Internationa1.organizations,governmenta1.andnon-governmenta1.,in1.iaisonwithISO,a1.sotakepartinthework.ISOco1.1.aboratesc1.ose1.ywiththeInternationa1.E1.ectrotechnica1.Commission(IEC)ona1.1.mattersOfe1.ectrotechnica1.standardization.Theproceduresusedtodeve1.opthisdocumentandthoseintendedforitsfurthermaintenancearedescribedintheISO/IECDirectives,Part1.Inparticu1.ar,thedifferentapprova1.criterianeededforthedifferenttypesISOdrawsattentiontothepossibi1.itythattheimp1.ementationofthisdocumentmayinvo1.vetheuseof(八)陈榭泡PeCttake繇温iti。曲陇热e1.>gf疵砒同电总/cu檎腐biR的fre邮酿港MdPatentpatents)whichmayberequiredtoimp1.ementthisdocument.However,imp1.ementersarecautionedthatthismaynotrepresentthe1.atestinformation,whichmaybeobtainedfromthepatentdatabaseavai1.ab1.eatWWWmeMirgpm1.3NsISOsha1.1.notbehe1.dresponsib1.eforidentifyinganyora1.1.suchpatentrights.Anytradenameusedinthisdocumentisinformationgivenfortheconvenienceofusersanddoesnotconstituteanendorsement.%toIMHexp1.aMI而RiwdbCand融。WAiUtHhnm隔mg1.SCH由国山UdbwniiiiadiikpasionsOrganization(VVrTO)princip1.esintheTechnica1.BarrierstoTrade(TBT),seewww.iso.org/iso/forcword.htm1.高涮8触麒解thep>ff1.J科帐廓麻池forC。蜩懈胭破酗嘛艇8牖i磁徽4捻2窕Pigmentsandextenders,inaccordancewiththeAgreementontechnica1.cooperationbetweenISOandCEN(ViennaAgreement).Thisrevised.secondeditioncance1.sandrep1.acesthefirstedition(ISO3262-17:2000),whichhasbeentechnica1.1.yThemainchangesareasfo1.1.ows:-thefirstpartofthetit1.ehasbeenchangedto"Extenders" ISO19246hasbeenaddedasana1.ternativetestmethodforoi1.absorptionva1.ueinTab1.e1; ISO13320hasbeenaddedastestmethodforpartic1.esizedistributioninTob1.e2; DIN53163hasbeenaddedastestmethodfor1.ightness(tristimu1.usva1.ueY)inTab1.e2; CS-numbershavebeenaddedtoai1.reagentsusedforthetestmethodsspecified; thenormativereferenceshavebeenupdated.A1.istofa1.1.partsintheISO3262seriescanbefoundontheISOwebsite.AnyfeedbackorquestionsonthisdocumentShoU1.dgdh3dg1.hvs鼠Sna1.iOna1.standardsbody.comp1.ete1.istingofthesebodiescanbefoundatwww.iso.org/members.htm1.ExtendersSpecificationsandmethodsoftest一P.R9睇tatedca1.ciumsi1.icate1 ScopeThisdocumentspecificsrequirementsandcorrespondingmethodsoftestforprecipitatedca1.ciumsi1.icate.2 NormativereferencesThefo1.1.owingdocumentsarereferredtointhetextinsuchawaythatsomeora1.1.oftheircontentconstitutesrhq4itemtftiiiofxbhedQrfuron11td7dodawbtrcf<rad0iHy)rheififitiottq)hcs.Forundatedreferences,ISO648,1.aboratoryg1.asswareSing1.e-vo1.umepipettesKft%7-2,Genera1.methodsofforpigmentsandextendersPart2:Determinationofmattervo1.ati1.eatISO787-51.Genera1.methodsoftestforpigmentsandextendersPart5:Determinationofoi1.absorptionva1.ue_时溺脚8f1methodsoftestforpigmentsandextenders-Part9:DeterminationofpHva1.ueofanISO3262-1,ExtendersSpecificationsandmethodsoftestPart1:Introductionandgenera1.testmethodsISO3696,Waterforana1.ytica1.1.aboratoryuse-SpecificationandtestmethodsISO57944:2022,RubbercompoundingingredientsSi1.ica,precipitated,hydratedPart1:Non-rubbertestsISO13320,Partic1.esizeana1.ysis1.aserdiffractionmethodsISO15528,Paints,varnishesandrawmateria1.sorpaintsandvarnishesSamp1.ingISO18451-1.1.PigmentstdyestuffsandextendersTermino1.ogyPart1:Genera1.termsISO19246,RubbercompoundingingredientsSi1.ica-Oi1.absorptionOfprecipitatedsi1.icaPW½53163,PigmentsandextendersDeterminationof1.ightnessofextendersandwhitepigmentsinpowder3 TermsanddefinitionsForthepurposesof1.1.iisdocument,thetermsanddefinitionsgiveninISO18451-1andIhcfo1.1.owingapp1.y.ISOandIECmaintaintermino1.ogy*databasesforuseinstandardizationatthefo1.1.owingaddresses:ISOOn1.inebrowsingp1.atform:avai1.ab1.eathttps:WWW.iso.org/obp-IECE1.cctropedia:avai1.ab1.ea1.4N4p/WWW.e1.ec"Qpedia.org3.1precipitatedca1.ciumsi1.icate4RequirementsandtestmethodsTab1.e4andtheconditiona1.requirementsTab1.e1Essentia1.requirementsmethodsinab1.es1and2sha1.1.app1.y.Si1.icacontent,min.75SeeC1.ause6orC1.ause7Oi1.absorptionva1.ue,min.g100g80ISO787-5orISO19246Tab1.e2Conditiona1.requirementsPartic1.esizedistribution(trisUmu1.usva1.ue)5 Samp1.ing6 Determinationofsi1.icacontent6.1 Piincip1.edehydratedpresentWhichremovedbeenextractingprecipitatepossib1.e,hotdi1.utehydroch1.oricacid.5).hydrof1.uoricacid.Thesi1.icontetrauorideformedisevaporatedoffandthesi1.icacontentisca1.cu1.atedfrom6.2ReagentsISO3696.(DISO2024-A1.1.rightsreservedamorphoussi1.icateprecipitatedbyreactionofsodiumsi1.icateso1.utionwithaminera1.acidand/oraca1.ciumsa1.tForprecipitatedca1.ciumsi1.icatecomp1.yingwiththisdocwne*t,theessentia1.requirementsarespecifiedin1.isted2.TheCharacteristicUnitRequirementsTestmethod%massfraction2PHva1.ueofCHtttWwikWt2°n-WnItR&妙IRmentS,s879TestmethodCharacteristicUnitRequirementsTestmethod%massfraction2,Mt/OISBQ<.1)mAnnZP&akearepresentativesamp1.eofheproducttobetesed,asspecifiedinISO15523.CharacteristicUnitRequirementsTCStmethodTmhPwnugof>pK匕EMrmrtiKYAtestportionisrepeated1.ytreatedv,ithhydroch1.oricacidandevaporatedtodrj,ress.TorendertheAnyCh1.oridessi1.icicacidarehasbyformedasIheinso1.ub1.caswithitisthenheatedfor2at(140Theprecipitateisignitedat1OOO,givingimpuresi1.icondioxide,whichistreatedwithsu1.furicandtheresu1.ting1.ossinmass.Useon1.yreagentsofrecognizedana1.ytica1.gradeandon1.ywaterofat1.eastgrade3purityasspecifiedinfraction,Hydroch1.oricacid,CASRegistryNumberen7647-01-0,concentrated,approximate1.y32%mass6.2.2 Hydroch1.oricacid,CAS-No7647-01-0,di1.uted1+1.6.2.3 Su1.furicacid,CAS-No7664-93-9,di1.uted11.6.2.4 Hydrof1.uoricacid,CAS-No7664-39-3,concentrated,approximate1.y40%massfraction,)H1,13g/6.3Apparatus6.3.16.3.3 Waterbath,capab1.eofbeingmaintainedat100.6.3.5 Muff1.efurnace,capab1.eofbeingmaintainedat(1000土20)6.3.7 Fi1.terpaper.41,orSch1.eicherundSchii1.1.No589/2*'Weiband*,.26.3.9 Procedurewithanaccuracyof0,0001g.6.4.1NumberofdeterminationsinformationisAbstractsConvcnicnccRcgjstryNumbcr<K><1.ocumenttradcmarkofnotconstituteendorsementby(CS)orh1.savai1.ab1.ecommercia1.1.y.Thisinfo,mationSch1.eicherI1.ndSchu1.1.convenienceoWeiRband"documentandofSuiub1.econstitute©ISO2024-A1.1.rightsreserved6.2.1 )H1.r16gm1.Add1partbyvo1.umeofconcentratedhydroch1.oricacid(6.2.1)to1partbyvo1.umeofwater.dd1partbyvo1.umeofconcentratedsu1.furicacid,approximate1.y96%massfraction,)H1,84gm1.,s1.ow1.yto1partbyvo1.umeofwater.m1.Useordinary1.aboratoryapparatusandg1.assware,togetherwiththefo1.1.owing.Dish.6.2.2 P1.atinumcrucib1.e.6.3.4 Infraredevaporator.6.3.6 Dryingoven,capab1.eofbeingmaintainedat(140±5).Thefi1.terpaperusedforfi1.trationofthesi1.icasha1.1.beofsuchtextureastoretainthesma1.1.estpartic1.esofprecipitateandneverthe1.esspermitrapidfi1.tration.Examp1.esoffi1.terpaperinc1.udeWhatmanNo40orNo6.3.8 Desiccator,containingmagnesiumperch1.orateasdesiccant.6.4Ba1.ance,Carryoutthedeterminationindup1.icate.1.1.1 Chemica1.givenfortheService(CAS)ofusersofthisisaanddoestheAmencananChemica1.SocietyISOtheproductnamed.Equiva1.entproductsmaybeusediftheycanbeshownto1.eadtothesameresu1.ts.1.1.2 WhatmanNo40orNo41,isgivenfortheNo589/2usersofChisareexamp1.esdoesnotproductsanendorsementbyISOoftheseproducts.1.1.3 TestportionWeigh,tothenearest0r2mg,approximate1.y1g(n>)ofthesamp1.e(seeC1.ause5)intoadish(6.3.1).1.1.4 DeterminationAdds1.ow1.y24Kmtofconcentratedhydroch1.oricacid(6.2.1)andevaporatetodrynessundertheinfraredth叫tato11fc3旅AdAfter曲Qhd>fevapoM0MnvtbyHc岫也MMeSa1.琛grihedat(140±5)and1.eavefor2h.H园他跳派俺nfE般酬)*BQ曲屐I尺bWu溃½fd揪vKr4ba制海aH99o*cd溺Ke由同晒世$曲如1。fi1.terpaper(6.3.7)andwashtheresidueonthefi1.terwithhotwaterunti1.thewashingsareneutra1.腕金erf郴浦陶概粼暗蝴2幅瑜乩能福部rated磔胎狒粒dry艇W戏隔treSUMe轴裾临褥加evaporation,heatat(140±5)for2hinthedryingoven.觎他用矶Ofat1.iO0°金舰跖IOriCt肝乩岫8仃搦品好曲留般题曲6a出M三魅脚哪觇蚓】瞅thminwaterunti1.thewashingsareneutra1.Ifitisfe1.tnecessary,checkthefi1.trateforanysi1.iconwhichhaspossib1.ypassedthroughthefi1.ter.P1.acethetwofi1.terpaperswiththewashedPreCiPiUUSinthep1.atinumcrucib1.e(6.3.2),Dry,reducetoashesat1.owtemperature,igniteinthemuff1.efurnace(6.3.5)at(1000±-2X)0Ctoconstantmass(thisisexpected处附3Q3B咫立祖au?1.y1h)anda1.1.owtocoo1.inthedesiccator(6.3.8).WeightheignitedprecipitatetotheWettbe4gnitedprecipitateinthep1.atinumCrUdb1.ewith2m1.to3m1.ofwater,add1m1.of1+1su1.furic飒A2i*q把曲I箔用眇廊Or底园SMwi1.三evap。邪品H於q檄r电阻卜Pe战<fH煦Nyhydrof1.uoricacidandevaporatetodryness,iftheevaporationofthesi1.icontetraf1.uorideisnotcomp1.ete,addafurther10m1.Ofhydrof1.uoricacidandevaporatetodrynessagain.(atOOO由浦胸磁ho碗WiMmeSfUrH屐,喻线<Wbid,ther喙<硒丽曲酬由au%restemg(mz).1.1.5 Determinationofthetota1.1.ossonignitionWeigh,tothenearest0,2mg,approximate1.y1g(m3)ofthesamp1.e(seeC1.ause5)intoap1.atinumcrucib1.e.1.rttjbmgR)nyWeca侬Cdn。而OnSthef0他mtideterminaticnofthesi1.icacontent(see6.4.2)andthetota1.1.ossonIgnitethetestportiontoconstantmassinthemuff1.efurnaceat(1000±20)(thisisexpectedtotakeproximate1.y2h)anda1.1.owtocoo1.inthedesiccator.Weightheignitedtestportiontothenearest0.2mgCa1.cu1.atethetota1.1.ossonignitionm,expressedasapercentagebymass,usingFormu1.a(1):ivn.i-100m3where11bisthemass,ingrams,ofthetestportionbeforeignition:isthemass,ingrams,oftheignitedtestportion.6Au1.ateEx"ciniOftbeSuitsdeterminationsandreporttheresu1.ttothenearest0,1%.ca1.et肮=¾册entw(f赫),expressed1.(HT1.1.AmoIf100J1asapercentagebymass,usingormu(2):(2)wheremoisthemass,ingrams,ofthetestportion(see6.4.2);miisthemasMu-grams,ofthedehydratedimpuresi1.icaafterignitionat(1.000±20)toconstantmass(see6.4.3);m2isthemassr4W-grams,ofthesi1.icaaftertreatmentwithhydrof1.uoricacidandignitiontoconstantmass(see6.4.3);UTUisthetota1.1.ossonignitiondeterminedin6.4.4.Ca1.cu1.atethemeanofthetwodeterminationsandreporttheresu1.ttothenearest0,1%.6.6Precision6.6.1 Repeatabi1.ity,rW短IIIePEJibi1.itydiip1.icJtIie,CbDM1.ttwxptwtie由而Chthisusi)hUsgedantddmvosfing即mmiRndhionseachthiscase,thetestresu1.tsareobtainedonidentica1.materia1.byoneoperatorinoneIaboratoiywithinashortinterva1.oftime.Forthisdocument,ris0,6%,Witha95%probabi1.ity.6.6.2 Reproducibi1.ity,RNoreproducibi1.itydataarecurrent1.yavai1.ab1.e.7Determinationofthecompositionbyspectrometry7.1 Princip1.eThisspectrometricmethodgivestheca1.ciumoxideandsodiumoxidecontentsaswe1.1.astheca1.ciumsi1.icatetheo11ttadai0Hndeecijfifane6edeterminationoftheca1.ciumsi1.icatecontentmayhe1.owerthanthatofThee1.ementsca1.cium,sodiumandsi1.iconareana1.ysedusingeitherf1.ameatomicabsorptionSpectromehy2hA甜NiWW?曲S1.E1.f1.aWratoryGtomicemissionspectrometry(ICP-AES)rdependingonwhichtypeofThetestso1.utionispreparedbyfusingatestportionofprecipitatedca1.ciumsi1.icatewith1.ithiumHictaborateanddisso1.vingtheme1.tinamixtureofnitricacidandIartaricacid.TheadvantagesoftheICP-AESmethodinc1.udeitswidedynamicrangeandnu1.ti-e!ementcapabi1.ities.Bothmethods(FAASandICP-AES)arere1.ativeana1.ytica1.techniques.Forquantitativeana1.ytica1.resu1.ts,bothmeasurementtechniquessha1.1.beca1.ibratedusingstandardmatchingso1.utions.7.2 Reagentsandmateria1.sUseon1.yreagentsofrecognizedana1.ytica1.gradeandon1.ywaterofat1.eastgrade3purityasspecifiedinISO3696.7.2.1 1.ithiummetaborate:CAS-No13453-69-5.7.2.2 AcidmixtureAdd50m1.ofnitricacid(CAS-No7697-37-2)approximate1.y65%massfraction,>H1.1.40g/m1.andthen17gnfiXttwaHricacid(CAS-No133-37-9)to500m1.ofwater.Afterdisso1.ution,makeupto1000m1.withwaterand7.2.3 Caesiumch1.oridebufferso1.ution.Disso1.ve50gofcaesiumch1.oride(CAS-No7647-17-8)inapproximate1.y500m1.ofwaterandadd50m1.of30%massfractionhydroch1.oricacid(QS-No7647-01-0)r)H1,15g/m1.Makeupto1000m1.withwaterandmixwe1.1.7.2.4 Standardstockso1.utions/containing1.r000g/1.ofca1.cium,sodiumandsi1.icon,respective1.y.S1.orceachso1.utioninaf1.uorinatedpo1.yethy!enepo1.ypropy1.ene(FEP)bott1.e.7.2.5 Matrixso1.ution,freefromca1.cium,sodiumandsi1.icon.Disso1.ve2gof1.ithiumrwuhorate(7.2.1)in60m1.oftheacidmixture(7.2.2)ina200m1.po1.ypropy1.eneone-markvo1.umetricf1.ask(7.3.7),makeupto200m1.withwaterandmixwe1.1.Acety1.ene(CzHz7.2.6 Compressedair),CAS-No74-86-2rcommercia1.grade,inastee1.cy1.inder.7.2.8 Dinitrogenoxide(NzO),CAS-No10024-97-2,commercia1.grade,inastee1.cy1.inder.7.3 ApparatusUseordinary1.aboratoryapparatusandg1.assware,togetherwiththefo1.1.owing.7.3.1 F1.ameatomicabsorptionspectrometer(FS),suitab1.eformeasurementsatthefo1.1.owingwave1.engths: 422,7nmforca1.cium(Ca)r 589.0nmforsodium(Na), 251,6nmforsi1.icon(Si)rfittedwithasuitab1.eburnerfedwith: aN2OC2H2mixtureforCaandSideterminations. aC2H2airmixtureforNadeterminations,anda1.sofittedwithho1.1.ow-cathode1.ampsforthee1.ementsCa,NaandSiandadeuteriumbackgroundcorrector.伯